Process of extracting oil from cottonseed



R. o. BoY'KlN YROCESS OF EXTRACTING OIL FROM COTTON SEED mea uw. a, '1925 QQIN QQWQIN VSNN .N\Q m N 0 @s @u M@ w W WQ E O Y WNY ww ,VN W MH m 1 ml c f M @Q M Sept. 9, 1930.

Patented SeptV 9, A1930 UNITED. STATES PATENT ori-"1ers ROBERT aBOYKIN, oF Los ANGELES, CALIFORNIA, AssIeNon 'ro N. RUSSELL vAIL,

-. for Los ANGELES, CALIFORNIA l PROCESS OF EXTRACTING OIL FROM COTTONSEED Application led December 8, 1925. Serial No. 74,005.

My` invention relates to the art of separating oil from organic matter, and it comprises a novel process in which the oil is expeditiously extracted from the organic matter. Solely for the purpose of illustration I elect to show and describe my* invention as being used for treating cottonseed-meal and extracting oil therefrom, but I do not intend to limit my invention to this onel embodiment 1o since it is applicable to use upon other oilbearing matter,

In the process of extracting oil from cottonseed, it is common practice to grind the seed and to mix it with a solvent in order to dissolve the oil from the solid constituents of the seed. The pregnant oil (solvent carrying dissolved oil) is then extracted fromthe solids of the meal, usually by a vacuum filter, and the pregnant solvent is then Jtreated to separate it intol organic oil and solvent.

I have found that the'pregnant solvent is not separated from the solids as rapidly' as it might be, by the vacuum filter, by reason of thepresence of vglutinous or colloidal sub-` v'stances which clog the vacuum filter. These glutinous substances are albumin or proteins in mostv cases. y

I have discovered that ,the cottonseed-'meal can be treated to render these glutinous sub- .to stances ilfsoluble or granular so that they 'are non-adhesive and non-colloidal. Y Cottonseed meal, thus treated, may have pregnant solvelitI more quickly and elciently separated fromthe solids.l y a `It is therefore an lobject of this invention' to provide an extraction'process is superior to others because of its quicker and more eficient operation.

It is another obj eet of this invention to proi vide a process of this character in which the ganic matter .is so treated that glutinous.

or su stances are coagulated and made insoluble and granular. f l l Other .objects and advantages of this in-r vention will appear in' the following description. v r

Referring to thepdrawing in which I diagrammatically illustrate'l an apparatus for conducting my invention, .1 is a fixer, 2 is a 5o mixer is a vacuum filter, 4 is a separator, 5

is a pre-heater, 6 is a still, 7 is an oil cooler,

'8 is an oil tank, 9 is a vapor cooler, 10 is a lvacuum pump, 11 1s a condenser and 12 is a condensate .'separator.

The fixer l'consists of a shell 12 having a l lthe interior o the shell 12 through the top 13. The paddles 16 operate to thoroughly mix the organic meal with the coagulating agent. The coagulating agent acts upon the glutinous substances of the meal and coagulates or converts these glutinous substances into insoluble and non-adhesive granules.

The meal is taken from the fixer 1 through a pipe 21 and is delivered to the mixer 2. The

pipe 21 is provided with a suitable screw feed4 '22. The mixer 2 consists of a shell 23 having a tight top 24 and a conical bottom 25. Mixing paddles 26 are placed inside the shell.` 23, being secured upon and operated by a shaft 27. The shaft 27 extends from the interior of vthe shell 23 through the'top 24 and has a pulley 28 secured-at the extending end thereof by means of which the shaft 27may be rotated. Solvent lis supplied to the mixer 2 by a solvent pipe 29 which connects to the interior of the shell 23 through the top 24. This solvent may be benzol, naphtha or any suitable hydrocarbon witha boiling point of from 120 to 250 F. and a specific gravity of approximatel .0.725. The organic meal is sup lied to t e, interior of the shell 23 throug the pipe 21 which connects near the upper part ofthe shell'23. 'In the mixer 2 the meal is thoroughly mixedfby means of the mixing paddles 26 with a so vent which is introduced into the shell 2 by means of the solventpipe 29. vThe solvent dissolves the organic oil from the meal during the mixing process and forms a pregnant solvent.

sol

The meal and epregnant solvent are taken from the mixer 2 by means of a pipe 31 and are delivered thereby 'to the filter 3. This pipe 31 connects to the mixer 2 at the cone bottom 25. .A screw feed 32 is provided in the pipe 31 for conveying the meal and solvent from the mixer 2 to the filter 3. The filter 3 consists of a housing 33 in which a filter drum 34 is rotatably mounted. This filter drum 34 is of standard Construction and the peripheral Wall thereof is formed of a porous or pervious Idrawn onto it,' by reason of the suction on the interior thereof, in a thin layer.' The vacuum on the interior of the drum 34 is effective in drawing the pregnant solvent from the meal or the'solidrconstituents of the organic matter.4 The insoluble granules which are formed from the glutinous vsubstances of the organic matter form a part of the solids which remain on the lter drum 34. A scraper 37 engages the periphery of the drum 34 and removes the solid constituents of the meal therefrom. The meal and the granules are directed through a chute 38 and are delivered by means of) a screw feed 39 to a suitable storage or for further treatment. A rewash solvent may be sprayed on the thin layer of organic meal on the drum 34 for rewashing same and assuring that all of the oil is removed therefrom. which rewash solvent may be supplied through a spray pipe 41.

The pipe`36 extends into -the upper end of a shell 42 of the separator 4. A vacuum pump 43 connects to the upper end of the shell 42 by means of a pipe44, by means of which vacuum pump 43 a vacuum is placed on the interior of the drum 34. The pregnant solvent taken from the solid 'constituents of the organic matter is drawn through the pipe 36 by the vacuum createdby the vacuum pump 43 and is delivered tothe shell 42. The pregnant solvent passes from the shell 42 through a pipe4 45 Whichconnects' to the lower end thereof. This pipe 45-extends down a short distance and is connected to a horizontal pipe 46 which connects to a' vertical pipe 47.

The pipe 47 extends to the preheater 5 and is connected to the lower end of a shell 51 thereof. The shell 51 is provided with intermediate heads 52 between vwhich pipes 53 extend. The pregnant. solvent is drawn throughthe pipes 45, 46 and 47 into the preheater 5" by means of a vacuum which is created by thevacuum pump 10. The man ner of connection of this vacuum pump 10 to theapparatus will be described shortly.

From the foregoing description it will be seen that the vacuum pump 10 provides a' vacuum which causes the pregnant solvent to flow through the pipes 45, 46 and 47 through the preheater 5 and into the still 6. The pipe 47 isof suflicient height so that oil cannot be entirely drawn therefrom. Therefore, there will always be a body of oil vat thel lower end of the pipes 47 and 45 which provides a vacuum seal whiclr prevents vacuum in both the preheater 5 and the still 6 from being destroyed. Thepregnant solvent passes into a space 'at the-lower end of the shell 51 and through the pipes 53 into a space at the upper end of the shell 51 and passes from the preheater 5 through a pipe A54. Steam or other heating agent is supplied to the interior of the shell v51 between the heads 52- and around the pipes 53 by means of a pipe 55 and is taken therefrom by means of a pipe 56.

The pregnant solvent is thus heated in the preheater 5 to a temperature which is higher than the boi-,ling point of the solvent. lVhen benzol is used, the temperature to which the pregnant solvent is raised inl the preheater is approximately 176 F.

The pipe54 conveys the heatedpregnant solvent to the still 6. The still 6 consists of a shell 61 which has a tight top 62 and a conical bottom 63. This shell 61 is filled with a multiplicity of ferrules or short lengths of pipe 64 which are placed in the shell 61 and allowed to have any position which they may occupy. The 'pipe 54 extends through the upper part of the shell- 61 and has a per-4 forated nozzle 65 provided at the end thereof which extends into the shell 61. Pregnant solventpis drawn in spray form through the perforated nozzle 65 onto the ferrules L64. The ferrules 64 are of various lengthsv and diameters and provide a very large surface` over which the pregnant solvent flows. This forms the solvent into thin films and exposes a maximum area of surface of the pregnant solvent. Steam preferably at a temperature of about 350 F. is admitted into the bottom of the still 6 through a plurality of nozzles 67 which connect to a steam manifold' 68, l

which manifold is supplied with steam by means of a pipe 69. The steam passes into the interior of the shell 61 and rises therethrough ina direction opposite to that of thefpregnant solvent which is flowing downwardly in the shell 61. In its upward passage the steam is brought into intimatecontactwith the pregnant solvent raising its temperature and 'causing arapid evaporationof the solvent therefrom so that 'the liquid -which reaches the bottom of the still-1.6 consists of oil which is substantially freef'ifromisolvent and free from deleterious substances.` Y

The oil is taken from thebott'onr'63 of the still 6 by means-of a pipe`j71iwhich-iconnects to one end of a shell 72 vfof-: theL-oilcoler 7.

The shell 72 is providedwith intermediate heads 73-between which pipes 74 are coni `nected. A cooling medium is supplied-to and takenv from the space inside the shell 72 be-l tween the heads 73 and around the pipes 74 by means of pipes 75. The oil passes from; the pipe 71 -into the space at one end v. of the the pipe 71 connects; and extends 'to the in-9 terior of an oilftank 8.` 'The pipe 81 has an end 82 which is arranged near the bottom' of the oil tank 8- so that itis kept submerged.

'By keeping the lower end 82 of the'pipe 81v submerged'a 'vacuum seal for thegbottom of .the still 6 is provided allowing oilvv to be deliv-jv ered to the loil tank 8 vwithout breaking the vacuum on the still 6., I .j

`The steam passing upwardfthrough the shell 61 and the solvent, vaporswhich are evaporated from'thepregnantisolvent are drawn from the shell 61 by a pipe 91 which connects to the vhead 62 lof: :the still 6.-- The `pipe 91 delivers the. vapors to the vapor cooler 9. The vapor cooler 9consists of a shell 92 having intermediate heads 93` between which pipes 944exte'nd. A coolingmedium is supplied to and taken from thespace in the shell 92 between the heads 93 and around the pipes 94by. pipes 95. Th pipe' 91 is connectedA to the upper end of the shell' 92 and delivers-vaporsinto 'a vspace at the upper end thereof. The vapors pass through the pipes 94 to a space.at-,-the lower endof i the shell 92, the vapors being considerably cooler 9. 1

reduced in temperatui'ea'nd partially condensed when' passing thxxj'ough the vapor The cooled vapors are delivered to the vac-I' uum pump 10 by a pipe .101'which connectsv to the lower end of the shell 92'and to the vacuum pump 10. The cooled'vapors are tak en from' the vacuum pump 10 by means of a pipe 111A er 11.

The condenser 1l consists of: a shell 112 having intermediate heads llbetween which heads l11? pipes 114 extend. condensing medium isfsupplied to the, spacejbetween the heads 113 and around the pipes 114 by means of pipes 115. The pipe 111 connects with a space provided at the upper yend of the shell 112 into which space the cooled vapors are passed. The cool vapors thereafter pass through the pipes 114 and into a space formed at the lower end o f the shell 112. The vapors are condensed into a liquid as they pass through the condenser 11. The condensats are taken from thelower lend of the condensandx are delivered to the condens-y er 11 by means of a pipe'121 and are delivered thereby to a condensate separator 12.

The steam condensates or water andthe solvent condensates `separate by gravity in .the condensate separator 12. The water is drawn from the separator 12 by a ,pipe 124 and condensed solvent is drawn from the sep-I ara-tor `12 by/a pipe 125.

Thevtemperature in the interior of the still Gis maintainedsuliiciently high by introduction ofvsteam'fat its lower end so that the pregnant solvent trickling downward through "the still Gis at all times heated to a temperature above the boiling point of the solvent.'

A certain amount of steam condenses into water in the still 6 and passes downward with the oil into the oil tank 8N Here the oil and water stratify, permitting them to be easily drawn ofi separately by suitable valved decanting pipes 126 vand 127 respectively which Klo are provided' at different levels ina side wall of the tank 8.

In the practice of my invention I prefer to use calcium/hydrate as a coagulating agent since it is effective in thoroughly coagulating albumins and otheru glutinous substances. The albumin may, of course, be rendered in- I soluble by the use of lother coagulants or by heating, for instance, by cooking for fifteen to forty minutes in a steam Jacketed vessel carrying a steam pressurg of from 20 to 100 lbs., without departing from the broad spirit of my invention. Otherjchemical coagulants which may be used in place of calcium hydrate with satisfactory-results are strontium hydroxide water, strong sodium chloride or calcium vchloride brine or acetic acid. The strengths of such reagents should be adjusted to the characteristics of the materials operated on, which the ordinary chemstean well do. Theclogging of the iilter 3 is done away with by such coagulation and the thoroughness and rate of filtration is increased. The

.- glutinous material which in previous prcesses would clog the porousmaterial of the ion V.filter drum and greatly impede' its operation iis entirely converted into a coagulated condition. This part lof my invention is an important advance in the art; since the ltration may take place more rapidly, and the organic matter may be more eiciently acted upon in the ilter 3.

-I desire to use benzol as a solvent because its boiling point is much lower than that of organic oil, and it may therefore be readil separated from the oil subsequent to iiltration.

By Wheating the pregnant solvent and separating'the solvent and oil in a high vacuum, I am able to carry certain undesirable constituents away in the solvent vapor and 'I am able to prevent a breaking down of the oil which, as is well known, would. form fatty acids and other deleterious substances.

- The undesirable constituents-of thef oil referred to above which are carried from the oil in the solvent vapor are generally of unknown composition. These undesirable compounds include certain amino acids, and they'are generally very .odoriferous and in the past have re uired a s ecial deodorizin rocess in order'to cxtractthem from the oil.

` -It is especially' desirable to apply the process of this inventionto th extraction of cottonseed oil from raw com inuted cottonseed.

-As an example ofthe application of this process to cottonseed, the process may be carriedy out with the following proportions of the' va-A rious materials involved. The cottonseed is first ground to a meal, 95% of which will pass /through a 200-mesh screen, and one part of this meal is mixed with .01 to ,O2 of a part of owdered calcium hydrate. yWhen the calciumI hydrate has been thoroughly mixed Fwith the meal, 1.25 parts of a suitable solvent,

`2o which may b e benzol, is added to the mixture of meal and calcium hydrate and the solvent;l v is thoroughly mixed ,withthe meal. The pregcottonseed in insoluble non-adhesive gran? ules,fadding a' low-boiling-point oil solvent insoluble in water to said cottonseed to dissolve said cottonseed oil which is disposed in the interstices between said granules. lter` ing'said oil dissolved in said solvent from said cottonseed, spreading Said pregnant solvent containing the dissolved oil in a thin lmin contact with steam for vaporizing said solvent, said steam being at a temperature and pressure ysuflicie'nt to vaporizcsaid sol vont but at which no'snbstantial `vaporization of said oil will occur, Witlnlrawing and condensing said vaporized solvent. :and removing said oil from contact with said steam.

In testimony whereof, I have hereunto set my hand at Los Angeles, California, this 2nd day'of December, 1925. I f y ROBERT '0. .BOYKIN :nant solvent is theiiilteredv from the mixture o andthe solvent and oil separated in the mank nerde'scribedabove.

It has been found advantageous in filtering l' the pregnant solvent from the meal to wash the meal by spraying as high as 1.7 5 parts of solvent upon the cake as it revolves pn the .all tlhe cottonseed oil which is present in the mea While my invention is particularly adapted for use" in the extraction of oil from cotton- 85 seed, it-may also be used with any organic material, and particularly vwith seeds ofv plants,such as beans and cocoanuts.

I claim as my invention: f l 1. A continuous process of separating cottonseed oil from raw comminuted cottonseed which consists in adding a chemical albumin coagulating agent to said raw, comminuted cottonseed so as to fix the albumins in said cottonseed in insoluble non-adhesive granules,

*adding benzol to said cottonseed to dissolve said cottonseed oil which is disposed in the interstices between said granules, ilterir 1g said oil dissolved in benzol from said cotwhichcons'ists in adding a chemical albumin f' coagulating agent tov said raw, comminuted 3Q filter drum 34. This insures the removal o f1 ltonseed,` and separating said benzol andsa'id 

